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Chemical engineering is an engineering branch that deals with the chemical production and manufacture of products that undergo chemical processes. This includes equipment design, creating systems and processes to refine raw material, as well as mixing, compounding, and processing chemicals to create products.
Chemistry and Chemical Engineering
Abstract
This study explores the influence of different counterions (K+, Na+, NH4 +) on the retention behavior of protonated basic solutes in chaotropic chromatography with hexafluorophosphate (PF6 −) in the mobile phase. The effects were analyzed at varying PF6 − concentrations and pH values, with experiments conducted at constant ionic strength using corresponding chloride salts (NaCl, KCl, NH4Cl) for consistency. Results show that counterions significantly impact the surface potential (Ψ0), affecting retention and elution sequences, enabling optimized separation. An empirical retention model, considering analyte structure and mobile phase composition, was applied. For solutes existing entirely as monocations, retention is primarily influenced by interactions with the electrical double layer on the stationary phase, regardless of ionic strength or pH. However, when analytes exhibit varying ionization states, both electrical double layer interactions and ion pairing with the chaotropic anion affect retention. This study underscores the potential of chaotropic chromatography for versatile separations of protonated basic analytes through careful selection of counterions and chaotropic anions. These findings enhance understanding of retention mechanisms, optimize chromatographic performance, and support the development of advanced analytical methods.
Abstract
Three techniques (UPLC, LC-MS/MS, and GC-MS) were developed to detect and evaluate various types of impurities in the trimetazidine API molecule. The UPLC method was developed to investigate simultaneously the nine process related impurities (IMP ‘A’ to ‘I’), GC-MS method was developed to quantify N-nitrosopiperazine and 1,4 dinitrosopiperazine simultaneously and LC-MS method for N-nitrosotrimetazidine quantification.
Every studied impurity had good linear calibration curves over the concentration ranges of LOQ to 150% of the test sample concentration. The developed approaches exhibited the ability to quantify investigated impurities with great sensitivity, as seen by the LOQ values obtained, which were much below the impurity specification limits. The specificity, linearity, sensitivity, accuracy, precision, and robustness of the devised approaches were all validated in conformity with ICH guidance. There was also discussion on the potential mechanism for the N-nitrosotrimetazidine synthesis.
This investigation showed that the established techniques (UPLC, LC-MS/MS, and GC-MS) for various forms of impurities in the trimetazidine API molecule may be utilised for quality control, as mandated by regulatory bodies to guarantee the product's safety in addition to effectiveness.
Abstract
The aim of this study was to design and evaluate a pesticide application system that is run from outside the greenhouse, reducing the operator's exposure to pesticides. The system included a network of pipes with fixed nebulizers distributed above the crop and equipment that injects the pesticide into the network. Seven nebulizers, three operating methods, two diameters, and four pipe lengths were evaluated using Christiansen's uniformity coefficient (CUC). The deposition of the system was evaluated, on the floor of a greenhouse without cultivation and on a tomato crop (Solanum lycopersicum), comparing it with a spray gun. The three-stage operation method, filling of pipes, application and surplus collection on return (LLA) was the most homogeneous. It was observed that a nebulization system composed of hydraulic nebulizers with a properly sized pipe network achieved similar deposition to gun applications. With the nebulization system the deposition at the top is greater than at the bottom of the plant.
Abstract
Sauchinone, a biologically active lignan derived from Saururus chinensis (family Saururaceae), demonstrates diverse biological effects, including alleviating jaundice, inflammatory disorders, hepatic steatosis, and oxidative damage. A rapid and selective UPLC-MS/MS method was developed and validated for quantifying sauchinone in rat plasma. Midazolam served as the internal standard (IS), and samples were prepared using ethyl acetate liquid-liquid extraction. Chromatographic separation occurred on a UPLC BEH C18 column with 0.1% formic acid and acetonitrile under gradient elution, completing each analysis within 3.5 min. An electrospray ionization (ESI) source in positive ion mode and multiple reaction monitoring (MRM) were used for quantification. Calibration curves were linear from 1 to 1,000 ng mL−1 for sauchinone in rat plasma. Intra-day and inter-day precision showed relative standard deviations (RSDs) below 13%, and method accuracy ranged from 89.0 to 109.8%. Mean extraction recoveries of sauchinone in rat plasma were 82.5–86.7%. This method was applied to evaluate sauchinone pharmacokinetics after intravenous (1 mg kg−1) and oral (5 mg kg−1) administration in rats, determining an absolute bioavailability of 4.3%.
Abstract
A simple, rapid, sensitive, and selective liquid chromatographic method using a tandem mass spectrometer was developed and validated for quantification of Bicalutamide in rat plasma, with Telmisartan as the internal standard (IS). The method employs protein precipitation extraction to isolate the drug and IS from rat plasma. Chromatographic separation was achieved on Waters XBridge C18 (75 × 4.6 mm ID, 3.5 μm particle size) column, using mobile phase consisted of acetonitrile (Phase A) and formic acid (Phase B) in an 80:20 v/v ratio, with a flow rate of 0.80 mL min−1 was employed. The set column oven and autosample cooler temperatures were 40 and 5 °C, respectively. The multiple reaction monitoring (MRM) transitions were m/z 429.08 → 254.90 for Bicalutamide and m/z 513.54 → 287.30 for the IS, providing high selectivity in the analysis. The method demonstrated excellent linearity and selectivity in the range of 0.995–1290.105 ng mL−1, with a lower limit of quantification (LLOQ) of 0.9 ng mL−1. The method met ICH guidelines for selectivity, sensitivity, precision, accuracy, and stability. The developed method has successfully applied to report the pharmacokinetic parameters of Bicalutamide in rats.
Abstract
Phellopterin, a naturally derived furanocoumarin, is widely distributed in medicinal plants like Angelica dahurica and Toddalia asiatica, as well as in citrus fruits. In this experiment, an UPLC-MS/MS bioanalytical method over the concentration range of 0.725–290 ng mL−1 was established for the quantitative analysis and pharmacokinetic study of phellopterin in rat plasma. Following protein precipitation with acetonitrile, the samples were separated by gradient elution on a UPLC system, using acetonitrile-0.1% formic acid as the mobile phase. Quantification was performed using multiple reaction monitoring (MRM) method in electrospray positive-ion mode (ESI+), with the ion transitions of m/z 301.1 → 233.4 for phellopterin and m/z 209.1 → 194.1 for the internal standard, fraxetin. The accuracy of phellopterin ranged from 87.9 to 112.4%, with the precision between 4.1 and 12.2%. The matrix effect was 92.4–97.4%, and the recovery was over 77.9%. The optimized UPLC-MS/MS bioanalytical method was successfully used to study the pharmacokinetics of phellopterin in rats. The AUC(0−t) values were 74.2 ± 7.9 ng mL−1*h for intravenous and 37.1 ± 5.3 ng mL−1*h for oral administration, while the corresponding half-lives (t1/2z) were 1.1 ± 0.2 h and 3.1 ± 0.7 h, respectively. The bioavailability of phellopterin was determined to be 16.7%.
Abstract
Berkeley rapid composting is one of the most effective ways of recovering organic waste, producing a final composting product in a very short time compared with other types of composting. For the first time in Morocco, and more specifically in Béni Mellal, this rapid composting process was applied to casing waste (50%) mixed with a manure fraction (50%) in order to study its qualitative and quantitative feasibility. The results of this experiment showed that the C/N ratio of the compost reached 21.3 and the quantitative efficiency did not exceed 47.9%. The aim of this work is to study the influence of the mixed fraction percentages and the effect of grinding the casings on the feasibility of rapid composting. The results showed that the economic efficiency of composting surpassed 60% when the casing fraction was more than 50% of the mixture and reached 65% when the casing waste was shredded.
Abstract
An analytical method based on ion-pair liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed to accurately determine neomycin B in bovine edible tissues (muscle, kidney, liver, fat) and milk. The pre-treatment procedure, including protein precipitation and solid phase extraction, was investigated to extract the analytes of interest better and remove matrix interferences. After sample pre-treatment, the 1% heptafluorobutyric acid 20 μL was added to the final extract. Then, the chromatography and mass spectrometry conditions were optimized, and the established method was validated. Good linearity (r > 0.999) was obtained at five matrices. The limit of detection, and the limit of quantitation were 10 and 20 μg kg−1, respectively. Trueness and repeatability at 0.5× maximum residue limit (MRL), MRL, and 2× MRL ranged from 96.67 to 109.54% and 3.36 to 9.01%, respectively. Adding the ion-pair agent to the extracts, rather than the mobile phase, ensures that neomycin B is efficiently retained on the reverse-phase column without contaminating the ion source. This simple and sensitive LC-MS/MS method is suitable for regularly monitoring neomycin residue in bovine edible tissues and milk.
The replacement of maize with grain sorghum is a promising practice for enhancing climate change adaptation strategies in the drought-prone areas of Central Europe. The refinement of the agrotechnics of commercial hybrids contributes to the development of sustainable agriculture. A field experiment was conducted between 24 May 2023 and 27 September 2023 in Keszthely (Hungary) in order to evaluate the effects of plant density (D1 = 240,000 plants ha–1, D2 = 280,000 plants ha–1) and equidistantly increasing N doses (0–40–80–120–160–200 kg N ha–1) on the grain yield, biomass weight and leaf area index (LAI) of 4 grain sorghum cultivars (G1 = KWS Nemesis, G2 = RTG Huggo, G3 = GK Erzsébet, G4 = ES Foehn). Another aim was to examine the effect of treatments on weed coverage. According to the results, plant density and N treatment had a general significant effect on grain yield (p < 0.05), biomass weight (p < 0.05) and LAI (p < 0.05; p = 0.015), regardless of the applied cultivar. Positive correlations were observed between biological and grain yield (D1: r = 0.9, p = 0.02; D2: r = 0.91, p = 0.01) as well as between LAI and grain yield (D1: r = 0.89, p = 0.6; D2: r = 0.91, p = 0.07). Significant differences were also observed between the grain yield (p < 0.05), biomass weight (p < 0.05) and LAI (p < 0.05) of the cultivars. In general, grain yields peaked around 120 kg N ha–1 at the plant density of 240,000 plants ha–1 and around 160 kg N ha–1 at the plant density of 280,000 plants ha–1. Among the experimental conditions RTG Huggo yielded the best results. In general, weed coverage was significantly lower (p = 0.002) in denser stands. The enhancing effect of N on weed coverage could not be detected (p = 0.318). In conclusion, a plant density of 280,000 plants ha–1, a N dose of 120–160 kg N ha–1 and RTG Huggo cultivar proved to be the best under the experimental conditions.
Abstract
The BET specific area (SBET), total pore volume and micropore volume were calculated to be 1319.36 m2 g−1, 0.686 cm3 g−1, and 0.636 cm3 g−1, respectively. ZIF-67 shows a type I isotherm for N2 adsorption-desorption. The ZIF-67 have particle size 614.9 nm with zeta potential equal to 5.52 mV (neutral surface) at pH 7, which indicates possibility of hydrophobic and π-π interaction between fipronil and ZIF-67. Fipronil adsorption with ZIF-67 was found to be monolayer and favourable, as evidenced by the Langmuir adsorption isotherm and endothermic and chemisorption process, as indicated by Pseudo second order (Ps.Sec.Ord.) kinetic model. The endothermic temper of adsorption was also concluded from the value of ∆Ho and ∆S i.e. 17.19 kJ mol−1 and 0.063 kJ mol−1 K−1, respectively. The ∆Go for adsorption of fipronil were found to be −1.293, −2.749, and −3.818 kJ mol−1 for 303, 318, and 333 K, respectively. Negative value of ∆Go shows feasibility and spontaneous nature of adsorption process. Under optimised conditions, ZIF-67 achieved 68.2% maximum removal of fipronil (20 mg L−1). Results obtained from the reusability studies suggested that ZIF-67 can be recycled by washing it five times with DMF and heating at 50 °C.
Abstract
Since the last few decades, the TLC has been an essential tool in the standardization and quality control of herbal medicines. Often, the traditional Thin Layer Chromatographic (t-TLC) profiling is inadequate in separating and identifying the huge numbers of phytochemicals present therein. A simple t-TLC is unable to accommodate or separate such large numbers of spots or bands on a plate. The present investigation has tried to adopt multidimensional and multiple development methods in combination to separate 21 phytochemicals and to generate a decisive chromatographic fingerprint of the sample. The most exciting point is that the qualitative profile generated here is highly reproducible for 19 phytocompounds. The limitations of traditional TLC in separating and identifying were overcome by the present investigation. The output of the present study may be an example of creating herboprint, which is generic and conclusive in the qualitative identification of complex herbal formulations. The most significant output of this work is that the presence or absence of any herb in a polyherbal formulation can easily be detected. It generates a unique herboprint, which can be referred as an authentic chromatographic fingerprint of the complex formulation. The concept adopted here is not new in the domain of TLC, but here maximized improvisation has been imposed in the field of herbs and herbal formulations. Significantly, a concept of coordinate position(s) which has been introduced is more rational than Rf value(s) for qualitative profiling in multidimensional development.
Abstract
Despite extensive development and widespread use, existing methods for analysis of caffeine and paracetamol overlook their environmental impact. Furthermore, these methods were not developed using the Analytical Quality by Design approach, leading to a significant gap in understanding critical separation factors. Moreover, the absence of a hydrophilic interaction liquid chromatography (HILIC) method for the simultaneous analysis of caffeine and paracetamol, integrating Analytical Quality by Design and a comprehensive green approach, presents an exciting opportunity for innovation and advancement in the field. In this paper, we report an efficient and sustainable HILIC method for caffeine and paracetamol analysis, which is based on Analytical Quality by Design, green and white chemistry principles. Optimal chromatographic conditions were adjusted using an InertSil Diol column with the mobile phase of acetonitrile and ammonium acetate buffer. The method was validated according to the International Council for Harmonisation guidelines, and its applicability in the analysis of Panadol Extra® tablets was confirmed. Relative standard deviation values were 0.07–0.28% for accuracy and 0.45–0.54% for precision. The environmental footprint and effectiveness of the method were evaluated through assessments of triple-color analysis which showed the dominance of green, blue, and white with scores of 0.66, 85.0, and 83.3, respectively. These parameters confirm that the method is eco-friendly, reliable, accurate, and precise for future use in the analysis of dosage forms containing caffeine and paracetamol. This is the first time that the Analytical Quality by Design approach has been combined with green and white chemistry principles, creating a strong synergy for the development of environmentally friendly methods.
Abstract
To investigate the determination of carbamazepine, oxazepine and their metabolites 10, 11-epoxy carbamazepine (CBZ), 10, 11-dihydro10-hydroxyl carbamazepine (MHD) in blood by HPLC and their interfering factors. The samples were pretreated by protein precipitation method. The chromatographic conditions were as follows: Agilent Eclipse Plus C18 column (4.6 mm × 250 mm, 5 μm); Mobile phase: acetonitrile-water (30–70); Flow rate: 1 mL·min−1; Column temperature: 37 °C; Uv detection wavelength: 210 nm. Based on common clinical antiepileptic drugs and serum samples of high bilirubin, high lipemia and low hemolysis, the anti-interference test was established. Under the chromatographic conditions, the separation of CBE, OXC and their metabolites was good, CBZ had a good linear relationship between 0.1 and 20 mg L−1 (r = 0.9994), and CBZE had a good linear relationship between 0.05 and 10 mg L−1 (r = 0.9998); OXC has a good linear relationship in 0.05–20 mg L−1 (r = 0.9993); MHD has a good linear relationship in 0.5–50 mg L−1 (r = 0.9995). The intra-day and inter-day precision RSD<13%, and the RSD of LLOQ<19%; the stability is good, the relative recovery rate is 91.17%–118.06%, and the method validation is in line with the “Chinese Pharmacopoeia” (2020 edition). Common clinical antiepileptic drugs, hyperlipidemia, and low hemolysis serum sample matrix have no obvious interference with monitoring, but high bilirubin serum sample matrix may have interference to varying degrees. The method is sensitive, accurate, simple, rapid and economical. It can be used for blood concentration monitoring and pharmacokinetic study of CBZ, OXC and their active metabolites.
Abstract
Rosuvastatin and ezetimibe, each with distinct mechanisms of action, have a well-established use in hyperlipidemia treatment. The recent adoption of their fixed-dose combination therapy has gained significant attention due to its enhanced therapeutic efficacy in managing hyperlipidemia and improved patient convenience. However, both active pharmaceutical ingredients (APIs) face challenges related to low bioavailability and non-selective action, highlighting the need for delivery systems able to target and control their release at the site of action. To overcome these limitations, lipid-polymer hybrid nanoparticles (LPHNPs) have been developed, leveraging the combined advantages of lipid and polymer nanocarriers for improved API delivery. This study focuses on the development and validation of a simple reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of rosuvastatin and ezetimibe in the developed LPHNPs, optimized to assess critical attributes of quality such as encapsulation efficiency (EE) and API loading capacity, which influence therapeutic outcomes.
Chromatographic separation was achieved by using a Zorbax Eclipse Plus C18 column and a mobile phase of diluted formic acid and acetonitrile (55:45, V/V) at a flow rate of 1.5 mL min−1. Detection was performed at 240 nm. The method was validated according to ICH Q2(R2) guideline, demonstrating excellent linearity, accuracy, precision and robustness.
The proposed method was used for the successful quantification of the EE and loading capacity of both APIs in LPHNPs, showing also potential for analysing their release profile by which valuable insights into their release mechanism and kinetics from the nanoparticle system could be obtained, and the stability of the designed delivery system as well, by providing effective assessment of API leakages from the LPHNPs over time, when kept at specific storage conditions.
Abstract
The preponderance of benign prostatic hyperplasia (BPH) and prostate cancer has increased in prevalence among aging men; prostate health management is becoming increasingly important. Studies indicate that substances such as beta-sitosterol and cholecalciferol may have therapeutic benefits for prostate disorders. This study aims to innovate the HPLC approach for the coexisting quantification of beta-sitosterol in Pygeum extract (Prunus africana) and cholecalciferol, providing a comprehensive strategy for evaluating the quality of herbal products targeting prostate health. The RP-HPLC technique was appraised using modified green star area (MoGSA) and BAGI metrics based on an Inertsil ODS-3 C18 column with a mobile phase of methanol and acetonitrile in a 95:5 ratio and detection at 210 nm. The strategy exhibited outstanding resolution, precision, and robustness, with a 12-min runtime. The method's linearity was confirmed with R 2 above 0.99, and the LOD and LOQ values were 0.61 μg mL−1, 0.76 μg mL−1, and 1.85 μg mL−1, 2.31 μg mL−1 for beta-sitosterol and cholecalciferol, respectively. Precision intra- and inter-day testing revealed RSD below 2%, confirming the method's reliability. Recovery studies indicated high accuracy, with recoveries of 101.50, 100.99, and 101.17, 100.92% in the pharmaceutical formulations and the supplement formulations for beta-sitosterol and cholecalciferol, respectively. This innovative dual-action approach may provide a promising therapeutic strategy by targeting multiple pathways involved in prostate function and disease prevention.
Abstract
The first targeted Rho-associated protein kinase 2 inhibitor was Belumosudil (Rezurock). After at least two systemic treatments failed for chronic graft-versus-host disease in adults and children aged 12 and older, belumosudil (BLS) was approved on July 16, 2021. This study established a validated Ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) system to estimate BLS in HLMs and assess metabolic stability. Agilent C18 column was used to separate BLS and encorafenib (internal standard) in HLMs using an isocratic mobile phase. The electrospray ionization (ESI) source produced BLS parent ions. Multiple reaction monitoring identified and measured BLS daughter ions. The methodology was validated following FDA standards that assessed linearity, selectivity, accuracy, sensitivity, precision, extraction recovery, matrix effects, and stability. The accuracy and precision ranged from −1.42 to 12.50% between days and from −0.89 to 10.5% within a day. The created BLS calibration curve displayed a linearity in the range from 1 ng mL−1 to 3,000 ng mL−1. The LLOQ of 0.64 ng mL−1 showed the method's sensitivity. The AGEE program displayed that the approach was eco-friendly. In vitro half-life and intrinsic clearance of BLS were 17.55 min and 46.21 mL min−1 kg−1, demonstrating a high extraction ratio drug. These features can improve the metabolic stability of new derivatives compared to BLS, making them important in medication design.
Abstract
The magnitude of the interactions between two phases may be deduced from results collected by various experimental techniques. One of them is Inverse Gas Chromatography (IGC).
The aim of the work was to compose and examine various polymer blends of PVC/PMMA, PMMA/PS and PVC/PS. Behavior of these blends was characterized by using the Flory-Huggins parameters estimated by means of the IGC. Based on the obtained results, the miscibility of the components in the tested polymer blends was determined. Characteristics derived from IGC data were compared with literature data calculated from equilibrium solvent (methanol) absorption.
Abstract
In this study, a simple, fast, and sensitive stability indicating CE method was developed for the quantification of Triamterene (TRM) and Hydrochlorothiazide (HCT) in pharmaceutical preparations. Detection was achieved using a photo diode array detector, and the separation process was conducted in a capillary with an inner diameter of 75 µm and a length of 40 cm. Optimum conditions were achieved by using a run buffer of 15 mM borate containing 20 mM SDS at pH 9.00, and applying a potential of 25 kV. HCT and TRM exhibited migration times of approximately 2.75 ± 0.007 min and 4.61 ± 0.022 min, respectively, under these conditions. The developed method was validated by assessing parameters such as linearity, selectivity, precision, accuracy, sensitivity, stability, and robustness. To assess the selectivity of the method, HCT, TRM, and tablets containing these compounds were exposed to acidic, basic, oxidative, thermal, and photolytic stress conditions. Ultimately, the method was proved successfully in accurately determining HCT and TRM levels in tablets.
Abstract
This study examined the effect of grapefruit seed extract (GSE) (0%–3%) on the stability of total phenolic content (TPC), anthocyanins, and colour in aronia juice under heat treatments (60 °C, 80 °C for up to 120 min). TPC and anthocyanins were measured using spectrophotometry and HPLC. The highest TPC (8545.02 ± 355.55 GAE mg L−1) was measured in aronia juice with 1% GSE after 60 min at 80 °C. The highest anthocyanin retention (3178.75 mg L−1) was detected in the sample with 1% GSE after 5 min at 60 °C. Cyanidin-3-galactoside was the most abundant anthocyanin, followed by cyanidin-3-xyloside and cyanidin-3-arabinoside. Cyanidin-3-arabinoside showed the lowest heat stability, while cyanidin-3-galactoside was relatively more stable. This study, the first to evaluate anthocyanin half-life values in chokeberry juice, suggests that 1% GSE enhances colour stability during heat treatment, supporting its use as a natural food additive.
Abstract
ASP3026 is a recently formulated and highly selective inhibitor designed to target the ALK kinase. ASP3026 efficiently inhibited ALK kinase activity and demonstrated superior selectivity at a panel of Tyr-kinases compared to crizotinib. The target of this investigation was to establish a highly accurate, fast, green, and highly sensitive Ultra-high performance liquid chromatography- Tandem mass spectrometry (UHPLC-MS/MS) technique for assessing the concentration of ASP3026 in human liver microsomes (HLMs). In vitro incubation, the metabolic stability of ASP3026 in HLMs was evaluated using this known approach. The validation steps for the UHPLC-MS/MS analytical technique in the HLMs were performed along with the bio-analytical method validation guidelines settled by the US-FDA. To increase the ecological sustainability of the current UHPLC-MS/MS system, a lower flow rate of 0.3 mL min−1, a shorter elution duration of 1 min, and a reduced consumption of ACN have been implemented. A screening of the chemical structure of ASP3026 for hazardous alerts and metabolic lability was performed by the StarDrop package, that includes the DEREK and P450 modules. The analytical separation of ASP3026 and fenebrutinib (FNB) on the reversed phase Eclipse Plus C18 column was performed using an isocratic mobile phase approach. The calibration curve produced by the ASP3026 showed a linear association over the level range of 1–3,000 ng mL−1. A study was conducted to evaluate the precision and accuracy of UHPLC-MS/MS technology in evaluating both intra-day and inter-day variations. The accuracy exhibited a range of −1.56%–7.33% across various days, and a range of −0.78%–10.66% within the same day. The ASP3026 underwent in vitro half-life and intrinsic clearance measurements, yielding values of 14.32 min and 56.62 mL min−1 kg−1, correspondingly. According to in silico software research, using minor modifications to the piperazine component or substituting the group in drug design has the potential to improve the metabolic safety and stability of novel derivatives in comparison to ASP3026.
Abstract
In this experiment, ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was employed to quantify karacoline in mouse plasma following both intravenous and oral administration, thereby elucidating the pharmacokinetic characteristics of karacoline in mice. The analytes were extracted from mouse plasma using acetonitrile for protein precipitation. Chromatographic separation was performed on an HSS T3 column via gradient elution, with the mobile phase consisting of methanol and 0.1% formic acid in water. Quantification of karacoline and the internal standard (IS) was achieved using multiple reaction monitoring (MRM) mode. Six mice received an intravenous (i.v.) injection of karacoline at a dose of 1 mg kg−1, while another six mice were administered karacoline orally (p.o.) at a dose of 5 mg kg−1. The calibration curve for karacoline in mouse plasma ranged from 1 ng mL−1 to 2,500 ng mL−1. The intra-day precision was within 10.4%, and the inter-day precision was within 13.0%. Accuracy ranged from 89.1% to 107.5%, with recovery rates between 77.6% and 88.2%. Matrix effects were observed within the range of 77.6%–107.4%. This method successfully estimated the pharmacokinetics of karacoline, and its bioavailability was determined to be 27.2%, these are preliminary studies that require verification on a larger group of animals.
Abstract
An alternative to roller mills, a French-designed stone mill, was evaluated and compared with traditional laboratory roller mills through grinding performance. Developed by the Astrié brothers in the 1950s, the stone mill's slow-rotating granite stones purportedly preserve the full nutritional value of the grain. This study, conducted in collaboration with the Csoroszlya farm, compared flour from the same wheat batch ground by both an Astrié stone mill and a laboratory roller mill. Evaluations included the Pekar test for bran content, sieve analysis, measuring wet gluten content, and gluten index to assess protein quality. Rheological properties of the doughs were analyzed using Farinograph and Mixolab equipment, which indirectly also measured amylase enzyme activity. Results indicated that the stone mill produced flour with finer grain size, higher protein content, and higher enzyme presence, although challenges remain in achieving optimal gluten index and dough stability.
Abstract
In this study, a simple, rapid, and sensitive capillary electrophoresis (CE) method was developed that allows simultaneous analysis of zonisamide (ZNS), rufinamide (RFN), and lamotrigine (LMT) in pharmaceutical preparations. This study introduces the first application of CE for the simultaneous determination of ZNS, RFN, and LMT in pharmaceutical dosage forms. For the comparison a High-Performance Liquid Chromatography (HPLC) method was developed. In CE method, detection was achieved using a photodiode array detector (DAD) at a wavelength of 210 nm. A capillary with an internal diameter of 75 µm and an effective length of 40 cm was used for separation. The optimum conditions were achieved using 35 mM SDS, 6 mM borate, 10 mM phosphate buffer (pH 9.00) containing 5% isopropyl alcohol (IPA), and applying a potential of 15 kV. Under these conditions, the migration times of ZNS, RFN and LMT were observed to be 5.99 min, 6.77 min and 8.46 min, respectively. In HPLC method, detection was achieved using a photodiode array detector at a wavelength of 210 nm. A C18 column (4.6 × 100.0 mm, 3.5 µm i.d.) was used for separation, with a mobile phase consisting of acetonitrile and pH 4.0 50 mM phosphate buffer (18:82, v/v) at a flow rate of 1.0 mL min−1. In this method, the retention times of ZNS, RFN and LMT were observed to be 6.41 min, 7.29 min and 4.95 min, respectively. The validity of the developed methods was examined through parameters such as linearity, precision, accuracy, sensitivity, stability, and robustness. In CE method, the limit of detection (LOD) values for ZNS, RFN and LMT were calculated as 0.035 μg mL−1, 0.016 μg mL−1 and 0.007 μg mL−1, respectively. For HPLC method, the LOD values were determined as 0.003 μg mL−1, 0.002 μg mL−1 for RFN and 0.001 μg mL−1 for LMT. Both developed methods were successfully applied to pharmaceutical dosage forms and shown to be compliant with United States Pharmacopeia (USP 47 - NF 42). In conclusion, both methods developed in our study yielded comparable results in terms of robustness and analysis time. HPLC demonstrated higher sensitivity compared to CE and is preferred for analyses at very low concentrations, while CE is ideal for green chemistry applications due to its minimal solvent and sample consumption.
Abstract
Violanthin, a compound isolated from the stems of Dendrobium officinale, exhibits potent antioxidant and antibacterial activities. However, no research has been conducted on the identification of violanthin in mouse plasma using UPLC-MS/MS. The present study aims to develop a selective UPLC-MS/MS method for the quantification of violanthin in mouse plasma. Samples were prepared using acetonitrile for protein precipitation, with aconitine as an internal standard (IS). Chromatographic separation was achieved on a UPLC HSS T3 column with acetonitrile and 0.1% formic acid as the mobile phase. Quantification was performed in multiple reactions monitoring (MRM) mode, targeting fragment ions m/z 579.6→457.2 for violanthin and m/z 646.6→586.5 for IS. Mouse blood samples were collected at different time points following intravenous (4 mg kg−1) and oral (30 mg kg−1) administration of violanthin. The calibration plots for violanthin in mouse plasma exhibited a linear trend across the entire range of 5–2,000 ng mL−1, with both intra-day and inter-day precision RSDs below 10%. The bioavailability was determined to be 24.3%. This UPLC-MS/MS method effectively facilitated pharmacokinetic studies of violanthin in mice.
Abstract
The determination of total flavonoid content (TFC) through the aluminum chloride (AlCl3) colorimetric test utilizing spectrophotometry is commonly used as a parameter for evaluating the quality of processes as well as food and herbal medicines materials. Nonetheless, it is laborious, lengthy, and necessitates substantial amounts of chemicals. This study aims to develop and validate the dot-blot assay with AlCl3 reagent for determining TFC in plant materials. In this method, the samples were not subjected to chromatography; instead, the plates were derivatized using AlCl3 in ethanol immediately after the application of samples and evaporation the solvent. The Al(III)-flavonoid complex was scanned (421 nm) using a TLC-scanner. The validation of the method was conducted on stability, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and robustness. The TFC of samples determined by dot-blot assay and spectrophotometry was subsequently analyzed using linear regression and Pearson correlation. The dot-blot assay for determining TFC met the stability parameter (RSD = 1.31–8.25%), intraday precision (RSD = 2.20–6.11%), inter day precision (RSD = 1.56%), linearity (r 2 = 0.9928), LOD (251.03 ng/spot), LOQ (760.71 ng/spot), accuracy (recovery = 70.81–75.61%), and robustness (RSD = 2.55 and 7.60%). There was a very strong positive linear relationship between the dot-blot assay method and spectrophotometry, with a linear regression coefficient of 0.9078 and a Pearson correlation coefficient of 0.911. The proposed method proved to be simpler, faster, and more economical for determining TFC. Thus, the method was beneficial in providing references for enhancing the quality control of food and herbal medicines.
Abstract
We developed and validated a liquid chromatography–mass spectrometry (LC–MS/MS) method for detecting conivaptan, an arginine vasopressin receptor blocker, in human plasma to facilitate future pharmacokinetic studies. After acetonitrile protein precipitation, analytes were separated on a Grace Alltima HP C18 reverse-phase column (5 μm, 2.1 × 50 mm), and gradient elution was performed using 0.1% formic acid and 5 mM ammonium formate in acetonitrile–water (1:9) and acetonitrile–water (9:1) over a 4-min run time. Positive-mode electrospray ionization and multiple reaction monitoring were applied. The assay was linear over the concentration range of 1–500 ng mL−1, with confirmed accuracy (intra-batch, 0.5–1.1%) and precision (intra-batch relative standard deviation [RSD], ≤5.7%; inter-batch RSD, ≤6.8%). Extraction recovery varied between 94.2–100.5%, and the matrix effect was 94.9–97.0%. To establish the stability, we examined plasma for 17 h at room temperature, 21 h at 2–8 °C, 57 days at −70 °C for three freeze-thaw cycles, and after processing for 52 h in the autosampler. We detected acceptable stability under all examined conditions. Hemolysis, hyperlipidemia, and dilution integrity satisfied the validation criteria. The method developed in this current study will help accurately quantify conivaptan in human plasma and define its clinical pharmacokinetics in the future.
Abstract
This work developed and validated a new UV-HPLC method for the separation and quantification of vonoprazan fumarate (VNP), amoxicillin (AMX), and clarithromycin (CLM), together in a ternary mixture and in laboratory-prepared tablets. A C18 column and a delightful 70:30 blend of 0.05 M KH2PO4 buffer pH 6 and acetonitrile were used as mobile phase. The flow rate was 1.5 mL min−1, while the wavelength of detection was 254 nm. Linear concentration ranges of (1.0–10.0 μg mL−1) vonoprazan fumarate, (1.0–125.0 μg mL−1) amoxicillin, and (25.0–1,200 μg mL−1) clarithromycin resulted in 0.061, 0.6213, and 7.302 μg mL−1 detection levels and 0.1849, 0.845, and 22.127 μg mL−1 quantification values for VNP, AMX, and CLM, respectively. The greenness of this method was evaluated using the National Environmental Methods Index assessment (NEMI), analytical Eco-scale Assessment (ESA) tool, Green Analytical Procedure Index assessment (GAPI), and Analytical Greenness metric assessment (AGREE), which authenticated the method to be eco-friendly. This method, which was systematically validated and used also to calculate the concentration of the three drugs in their dosage forms, showed high accuracy and precision. Additionally, it produced peaks that were clearly separated and resolved, demonstrating its robustness and specificity.
Soil organic carbon (SOC) levels directly affect the production and health of crops. Making use of a database of the usefulness of using the 350–2,500 nm Near Infra Red (NIR) spectroscopy data range on 200 soil samples from the Indian state of Uttar Pradesh was evaluated in this study. The more sophisticated Artificial Neural Network, to choose the spectral components that were used to forecast SOC, Random Forest (RF) and Ensemble Lasso-Ridge Regression (ELRR) were utilized. In the preprocessing, the inversion derivative, logarithmic(log) derivative, and logarithmic base to 10(log10x) derivatives were employed to duplicate the spectrum wavelength. The main characteristic of spectrum wavelength for SOC were found to be within the range of 350 and 450 nm, per the results. The best accurate estimation of SOC content was obtained by combining the suggested DSANN or Dropout Sequential ANN technique with the Log10x pre-processed data. The R-squared (R2), RMSE, and RPIQ (Ratio of Performance in Inter Quartile Distance) values for the testing dataset were 0.83, 0.08, and 4.32, respectively.
Abstract
The preservation of water resources is seriously threatened by the rise of pharmaceutical contamination. Ribavirin, a widely used antiviral drug, is among the pharmaceutical residues in wastewater. In this study, the adsorption capacity of activated carbon produced from tobacco stems, a by-product of the cigarette industry, was investigated. The produced activated carbon was characterised by BET, SEM-EDX and FTIR analyses. In the next step, removal of ribavirin from aqueous solutions using activated carbon was investigated. In the next step, the removal of ribavirin from aqueous solutions was tested with this activated carbon. Various factors such as initial ribavirin concentration (10–50 μg mL−1), solution pH (4–10), adsorbent amount (5–30 mg per 50 mL solution), contact time (0–150 min) and temperature (300–328 K) were investigated to determine the optimum adsorption conditions. Adsorption kinetics were investigated with first and second order pseudo models, and the equilibrium state was analyzed with Langmuir and Freundlich isotherm models. Thermodynamic parameters were calculated at different temperatures (300, 308, 318 and 328 K). The results show that a maximum removal efficiency of 91.83% was achieved at an initial concentration of 30 μg mL−1, adsorbent dose of 20 mg, contact time of 90 min and pH 7.00. The adsorption process was best described by the pseudo-second order kinetic model (R 2: 0.9987) and Langmuir isotherm model (R 2: 0.9971). Thermodynamic analysis shows that the process is spontaneous (ΔG < 0), exothermic (ΔH < 0) and causes a decrease in disorder in the system (ΔS < 0). This study reveals that tobacco stems can offer an environmentally friendly and economic treatment alternative.
Abstract
Aflatoxins (AFs) and deoxynivalenol (DON), common mycotoxins in cereals, pose contamination risks in beer production, often persisting from raw barley into final products. This study investigates the transfer and decomposition of AFs and DON during the barley steeping stage of malting. Barley spiked with AFs and DON was steeped, and mycotoxin concentrations were analyzed in both the barley residue and the resulting wastewater. Results indicated that AF and DON transfer into wastewater was influenced by water solubility, though concentrations remained below solubility limits. AFs and DON residues were also detected in the steeped barley. Decomposition studies showed that while AFs were partially degraded by UV light, DON required photocatalysis for effective degradation. However, matrix components in wastewater decreased the efficiency of DON decomposition, suggesting that preliminary removal of organic components from wastewater could enhance photocatalytic detoxification. These findings provide insight into mycotoxin management strategies for brewing wastewater, emphasizing the need for targeted pretreatment to improve degradation efficiency.
Abstract
The aim of the current investigation to estimate the amount of theobromine (THEOB), theophylline (THEOP) and caffeine (CAF) concurrently using ultra performance liquid chromatography with photo diode array detector (UPLC-PDA) in ultrasound assisted extract of commercially available food products. The commercially available products are categorized in three different groups including teas, coffees and chocolates. The UPLC approach is rapid, precise, highly sensitive and cost effective for the concurrent assessment of THEOB, THEOP and CAF in ultrasound assisted extract of commercially available food products. The mobile phase comprises a mixture of water and ACN (90:10, v/v) for the concurrent assessment of THEOB, THEOP and CAF in ultrasound assisted extract of commercially available food products. The current approach operated on a linear scale range of 6.66–33.3 ng mL−1, 3.33–33.3 ng mL−1 and 3.33 – 33.3 ng mL−1, respectively, for THEOB, THEOP and CAF at 272.5 nm wavelength. The LOD for THEOB, THEOP and CAF were assessed to be 1.10 ± 0.001, 0.75 ± 0.000 and 0.48 ± 0.002 ng mL−1, respectively by applying the present approach. The LOQ for THEOB, THEOP and CAF were assessed to be 3.35 ± 0.009, 2.29 ± 0.001 and 1.47 ± 0.001 ng mL−1, respectively by applying the present approach. These findings confirmed that the current UPLC approach is highly sensitive, accurate, precise and robust for the concurrent assessment of THEOB, THEOP and CAF in ultrasound assisted extract of commercially available food products. Antioxidant activity of different teas, coffees, chocolates as well as standard THEOB, THEO and CAF were determined by DPPH method.
Abstract
Osimertinib (Tagrisso, AstraZeneca Pharmaceuticals) is the inaugural third-generation irreversible EGFR-TKI that specifically targets both the EGFR T790M resistant mutation and EGFR-TKI-sensitizing mutations. On September 25, 2024, the Food and Drug Administration authorized osimertinib (OSM) for adult patients with locally advanced, unresectable (stage III) non-small cell lung cancer (NSCLC). The target of this work was to establish a fast, accurate, environmentally friendly, and highly sensitive UPLC-MS/MS methodology for detecting OSM levels in human liver microsomes (HLMs). The separation of OSM and zanubrutinib (ZNB) was accomplished utilizing a C8 column and an isocratic mobile phase. The linearity of the OSM calibration curve spanned from 1 to 3,000 ng mL−1. The AGREE score of 0.76 validates the efficacy of the current approach. The brief in vitro half-life (23.72 min) and moderate intrinsic clearance (34.18 mL min−1 kg−1) of OSM indicate that it resembles drugs with a moderate extraction ratio. The present LC-MS/MS technique is regarded as the primary analytical methodology for quantifying OSM in HLM matrices. The characterization of OSM metabolic stability and in silico ADME features are crucial for progressing the discovery of novel drugs with improved metabolic stability.
Abstract
Apples are among the most common fruits, produced on the territory of North Macedonia. Before they reach the market, it is essential to be tested for pesticide residues, which are used for protection against pests for this culture, and in order to ensure the customer safety. For this reason, a novel and simple method for simultaneous determination of captan, folpet, difenoconazole and chlorpyrifos in apple samples has been developed and validated. Acetone is used for extraction of the pesticide residues, followed by liquid-liquid (LLE) and solid–phase extraction (SPE). Separation and quantification of analytes is achieved on reversed-phase high performance liquid chromatography (RP-HPLC) with UV diode array detector (UV-DAD). The best results are obtained using analytical column LiChrospher 60 RP-select B (250 mm × 4 mm, 5 µm), with isocratic elution and acetonitrile/0.1 % acetic acid in water (70:30, V/V) as a mobile phase. The flow rate is 1 mL min−1, and UV detection is performed at 220 and 230 nm. The linearity of the method is tested in the range of 1.50–3.60 mg kg−1 for captan and folpet, and 0.35 – 0.60 mg kg−1 for difenoconazole and chlorpyrifos. The obtained values for recovery and RSD ranged from 94.94 to 114.63 %, and 0.09–9.25 %, respectively. The validated method is successfully applied to apple samples for the determination of the investigated pesticide residues.
Abstract
Aflatoxins, potent carcinogenic mycotoxins produced by Aspergillus species, persist in various foods, posing significant health risks upon consumption. This study assesses dietary aflatoxin B1 (AFB1) exposure in Vietnam using Margin of Exposure (MOE) and Hazard Index (HI) to evaluate risk levels in peanuts, chili powder, corn, and raisins. AFB1 levels were quantified by UPLC-FLD. AFB1 was detected in 71.5% of chili powder, 29.3% of peanuts, and 26.0% of corn samples, with no detectable levels in raisins. Peanuts and corn kernels were classified as high-risk, with MOE values below 10,000 (peanuts: 25.8–56.6; corn: 42.3–92.6) and HI values exceeding 1, potentially contributing to 20.4–44.7 and 12.5–27.3 liver cancer cases per 100,000 adults, respectively. In contrast, chili powder had MOE values between 3,208 and 7,021 and HI below 1, indicating a low public health risk. Raisins were deemed safe with MOE over 200,000 and HI at 0.01. Results also indicated higher cancer risk for women and lean individuals consuming the same AFB1 levels. These findings underscore the need for focused risk management strategies to mitigate AFB1 exposure and protect public health in Vietnam.
Abstract
In the field of pharmaceutical analysis, high-performance liquid chromatography (HPLC) is considered to be the key technique, which is one of the most efficient, quick, and easy methods for the simultaneous determination of two are more drugs. The purpose of the current study is to develop and validate the reversed-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of Paracetamol and Fexofenadine HCl. This approach was validated by the standards and The International Conference on Harmonization (ICH), and United States Pharmacopeia (USP) were followed in the development and validation of the method. The chromatographic conditions including a mobile phase comprised of a 35:65 buffer mix and acetonitrile with a 1.0 mL min−1 flow rate were used. A thorough investigation was performed, including linearity and range, specificity, robustness, accuracy, precision, solution stability, and system suitability. The outcomes of the studies have shown that, both Active Pharmaceutical ingredients i.e., Paracetamol and Fexofenadine HCl were separated in about 7.5 min. The variation coefficient for Paracetamol and fexofenadine HCl varied between 0.9992 R 2 and 0.9983 R 2, respectively. The devised method was proved accurate, as API recoveries in both cases of Paracetamol and Fexofenadine ranged from (99.79%, 100.72%, and 98.64%) to (99.96%, 100.64%, and 99.00%). The method's accuracy was further demonstrated by the solution stability which was 99.84% for Paracetamol, and 100.53% for Fexofenadine HCl. The suggested method for simultaneously measuring Paracetamol and Fexofenadine HCl was established, validated, and there was no evidence of any excipient interaction was observed.
Abstract
The need to develop environmentally friendly analytical approaches has driven the pharmaceutical industry to seek greener alternatives. Ultra-Performance Liquid Chromatography (UPLC) is known for its efficiency but traditionally relies on toxic solvents. Integrating Green Analytical Chemistry (GAC) principles aims to address environmental concerns while maintaining analytical performance. This work aims to advance and authenticate a green, efficient UPLC method for the concurrent quantification of Metformin (MET) and Empagliflozin (EPI) in tablet formulations, adhering to green chemistry principles and ensuring high analytical accuracy. The method was optimized using a UPLC-PDA system with a phenyl column and a mobile phase of ethanol and perchloric acid. Analytical Quality by Design (AQbD) was employed to optimize critical method parameters. Environmental impact was assessed using metrics such as GAPI, AMGS, and AGREE. Degradation studies under various stress conditions were performed to test method robustness. The method achieved high recovery rates for MET and EPI, with minimal interference from excipients. The environmental evaluation showed a high Analytical Eco-Score (AES) of 97, indicating low environmental impact. The AGREE score of 0.89 confirmed excellent alignment with green chemistry principles. Degradation studies confirmed the method's stability and reliability under stress conditions. The developed UPLC method demonstrates a significant advancement in analytical sustainability, offering an eco-friendly, efficient, and precise approach to drug analysis. The method's high alignment with green chemistry principles and its effectiveness in quantifying MET and EPI highlight its potential as a model for sustainable analytical practices in pharmaceutical analysis.
Abstract
Tea's beneficial effects have long been attributed to its abundance of natural bioactive compounds; however, the influence of variations in these compounds on taste and aroma remains poorly understood. To investigate the relationship between metabolomic profiles and tea processing adaptability, this study employed sensory evaluation and untargeted metabolomics to compare four tea cultivars from Guangxi—Ying Hong No.9 (YH), Gui Hong No.3 (GH), Gui Cha No.2 (GC), and Mei Zhan (MZ)—cultivated under the same conditions. Sensory evaluation revealed that GH and MZ exhibited the highest quality in green tea and black tea, respectively, while GC showed moderate quality, and YH performed less favorably than the other three cultivars. Metabolomics analysis uncovered significant differences in the metabolic profiles among the four tea cultivars, with MZ and YH displaying higher levels of flavonol glycosides, and GC and GH showing elevated levels of organic acids and fatty acids. Pathway analyses of GH and MZ indicated that the differentially enriched pathways were primarily related to linoleic acid metabolism and flavonoid and flavanol synthesis. Correlation analyses further revealed that the sensory quality of green tea was closely linked to fatty acids and organic acids in fresh leaves, whereas the sensory quality of black tea was strongly associated with flavonol glycoside levels. This study provides a comprehensive understanding of the complex relationship between metabolite characteristics and processing suitability in different tea cultivars, offering valuable insights into the development of tea germplasm resources in the Guangxi region.
Abstract
This research dealing with salting out TLC technique for simultaneous determination of two antihistaminic drugs Loratadine and its active metabolite desloratadine in pure, tablets and rabbit spiked plasma. Separation was performed on silica gel 60 F254 plates using aqueous ammonium sulfate and acetonitrile (6:4, v/v) as a mobile phase. The R f values were 0.51 ± 0.02 and 0.70 ± 0.004 for Loratadine and desloratadine, respectively in pure or dosage form while in spiked plasma R f values were 0.39 ± 0.004 and 0.61 ± 0.004 for both drugs respectively using levocetirizine as internal standard (R f 0.74 ± 0.004). The separated bands were scanned under UV light at λ 254 nm and the TLC chromatograms were captured by camera and treated with Image J software. Method validation was according to ICH and complied with USP31- NF26 guidelines. The correlation coefficients of calibration curves were 0.997 and 0.998 for Loratadine and desloratadine in pure and dosage form while in rabbit spiked plasma were 0.996 and 0.995 for both drugs respectively in the range 100–2,000 μg mL−1. limits of detection LOD and limits of quantitation LOQ for Loratadine and desloratadine were 7.84, 30.06 and 23.52, 91.18 μg mL−1 respectively as pure or as dosage form while LOD and LOQ in rabbit spiked plasma were 17.46, 14.03 and 52.38 and 42.09 μg mL−1 respectively.
Abstract
The automated system for enhancing plant growth presents an innovative approach to optimize quality of sugarcane cultivation for four main sugarcane growing zones. It includes issues like recommendation of crops based on soil nutrients, diagnosis of disease in the leaf and stem images of sugarcane, weed detection and harvesting time prediction. The research work proposed in the article presents an innovative two-stage approach for object detection and classification in agricultural imagery. Initially, YOLOv8 (You Only Look Once) is employed to accurately detect objects within images, delineating them with precise boundary boxes. Subsequently, the focus of hybrid model integrating Convolutional Neural Networks (CNNs) and Long Short-Term Memory (LSTM) networks, known as Contextual Long Short-Term Memory (CLSTM), is employed. This dual-stage methodology harnesses the speed and accuracy of YOLOv8 for robust object localization, while the CLSTM model ensures nuanced classification, contributing to comprehensive and accurate approach for object detection and crop-weed differentiation in agricultural scenarios. The proposed approach is compared with the four DL algorithms for identifying weeds in sugarcane crops and subsequently assessed their accuracy and F1 score performance. At a learning rate of 0.002, the findings of CLSTM showcase superior precision at 98.5%, recall at 97.8%, F1 score at 98.1%, and an overall accuracy of 97.7%. The subsequent task is harvesting time prediction, which entails identifying the best time to harvest sugarcane based on the planting period, weather predictions, and sugarcane brix value. The implementation of this automated system not only enhances the productivity of sugarcane cultivation but also serves as a model for sustainable and resource-efficient agriculture.
Abstract
Febrifugine, a potent quinazolinone compound derived from the Chinese herb Chang Shan (Dichroa febrifuga), exhibits diverse biological activities and has demonstrated anti-tumor effects by functioning as focal adhesion kinase (FAK) inhibitors. In this study, our objective was to establish a quantitative UPLC-MS/MS method and investigate the pharmacokinetic characteristics of febrifugine in rats following intravenous and oral administration routes. The rat tail vein was used for the collection of blood samples at designated time intervals following intravenous (2.0 mg kg−1) and oral (6.0 mg kg−1) administrations. Plasma samples were pretreated with acetonitrile as a protein precipitant and methylcytisine as an internal standard. Febrifugine concentration in rat plasma was determined using the UPLC-MS/MS method, and pharmacokinetic parameters were calculated using drug and statistics (DAS) software version for statistical analysis. The linear range of febrifugine in rat plasma was 1.5–1,500 ng mL−1, meeting the precision, recovery, and stability requirements for determination purposes. Febrifugine had a half-life (t1/2) of 3.2 ± 1.6 h after administered via intravenous route, while t1/2 was 2.6 ± 0.5 h after oral administration. The developed UPLC-MS/MS method is facile to operate while adhering to rigorous methodological verification standards, rendering it suitable for investigating the pharmacokinetics of febrifugine; and bioavailability was determined as 45.8%.
Abstract
This study presents the development and validation of a robust HPLC-UV method for the simultaneous detection and quantification of vitamin D2, vitamin D3, ergosterol, and 7-dehydrocholesterol in a single analytical run, adhering to ICH Q2 (R1) guidelines. Application of the HPLC-UV method to six vegetable oils demonstrated inherent vitamin D content and its enhancement under different radiation conditions. Oils were exposed to direct sunlight, UVA, and UVB radiation, with UVB showing the most significant impact on vitamin D levels. Notably, UVB exposure increased vitamin D3 in castor oil from 2.82 μg mL−1 to 4.29 μg mL−1 and vitamin D2 in mustard oil from 0.73 μg mL−1 to 1.89 μg mL−1. The findings highlight the potential of UVB radiation to convert vitamin D precursors to active forms more effectively than other radiation sources. This study provides a novel approach for naturally enriching vitamin D in vegetable oils, offering a promising strategy to mitigate vitamin D deficiencies in populations with limited sun exposure or dietary restrictions. The developed HPLC-UV method and resultant insights into the radiation-induced enhancement of vitamin D content in oils contribute valuable knowledge to nutritional science.
Abstract
Zanubrutinib (Brukinsa, BeiGene) is a FAD approved second-generation Bruton's tyrosine kinase inhibitor that has more selectivity and reduced off-target action, resulting in mitigated cardiotoxicity compared to ibrutinib. The target of this investigation was to establish a fast, precise, green, and extremely sensitive UPLC-MS/MS approach for quantifying the level of zanubrutinib (ZNB) in human liver microsomes (HLMs). The separation of ZMB and revumenib was achieved using C8 column and isocratic gradient of the mobile phase. The linearity of the constructed ZNB calibration curve was ranged from 1 to 3,000 ng mL−1. The StarDrop software package including DEREK and WhichP450 modules was used in screening for the toxic alerts the in silico metabolic lability of ZNB. The AGREE score was 0.76 that approves the greenness of the established method. The low in vitro t1/2 (17.61 min) and high intrinsic clearance (46.03 mL min−1 kg−1) of ZNB revealed that ZNB shares similarities with medications that have a high extraction ratio. The present LC-MS/MS approach is considered the first analytical methodology for assessment of ZNB metabolic stability in HLMs matrix. In silico data from WhichP450 and DEREK modules suggest that making small structural changes (bioisosteric replacement) to the carboxamide moiety during drug design can potentially improve the metabolic safety and stability of novel compounds relative to ZNB. These methods are essential for advancing the development of new pharmaceuticals, particularly in enhancing metabolic stability.
Abstract
Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. fruits (ESF) is a natural health food that has been widely used in traditional medicine. This study aimed to establish and validate a rapid and sensitive method for determining of six phenolic acids in plasma of normal and T2DM rats by ultra-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Separation and quantification were performed on a Waters HSS T3 column (100 × 2.1 mm, 1.8 μm) with water (A) and methanol (B). The electrospray ionization (ESI) source was operated in negative ionization mode. Multiple reaction monitoring (MRM) was used to quantitatively analyzed hyperoside m/z 463.2→301.1, caffeic acid m/z 179.1→135.1, chlorogenic acid m/z 353.2→190.9, gallic acid m/z 169.0→125.1, protocatechuic acid m/z 153.1→109.1, and isofraxidin m/z 221.1→191.0, respectively. The hypoglycemic effect of ESF was verified by determining blood glucose and lipid levels in a type 2 diabetes model. This study laid the foundation for exploring ESF clinical guidelines in the future.
Abstract
High Performance Thin Layer Chromatography has capacity to run many samples simultaneously and its reduced solvent usage. Simultaneous quantification of gallic acid, ferulic acid, rutin and berberine in Asthimajja Pachak Kwath has been developed and validated using a specific, precise, accurate, and low-cost high performance thin layer chromatography technique. Toluene: ethyl acetate: chloroform: methanol: formic acid (5:2:2:2:1, v/v/v/v/v) was used as mobile phase during separation, which took place on a stationary phase of pre-coated silica gel aluminum plate 60 F254. At 270 nm, separated components were densitometrically measured. The method was validated for linearity and range, precision, reproducibility, specificity, robustness, accuracy, limit of detection and limit of quantification as per International Council for Harmonization Q2 (R2) guideline. Gallic acid, ferulic acid, rutin and berberine regression coefficients (R 2) were found to be 0.9995, 0.9990, 0.9985 and 0.9997 accordingly. Gallic acid, ferulic acid, rutin and berberine percentage recoveries were measured to be 99.81 ± 0.833, 99.15 ± 0.776, 99.56 ± 0.582 and 99.90 ± 0.719 respectively. Having a reliable analytical method is essential for ensuring the quality, consistency, and efficacy of herbal formulations in traditional medicine. This meticulous approach is crucial for accurate quantification of the target compounds in the Asthimajja Pachak Kwath.
Abstract
Nowadays, drone imagery is a common way to quickly obtain information on the state of vegetation, as well as a method for taking orthophotos and terrain models. For terrain modelling, aerial photographs are required to have at least 60% overlap between adjacent images. Typically, the inadequate overlap is only discovered later, during post-processing. In our previous work we have presented a method we developed to determine on the spot, whether the in-flight images are suitable for producing the terrain model or whether it is necessary to re-render a part of the area, which can be done under the same conditions (weather, ionosphere, satellite geometry). Our proposed method for calculating the overlap is different from the usual procedure. Using VBA-based calculations, we computed the overlap between the images based on the position of the centre of the images, the altitude of the flight and the rotation angle of the images. The method was tested in practice, but we felt it necessary to verify our calculations. During the verification, we checked the VBA-based calculations using a Python script. The test showed that the results obtained with a previous midpoint calculation method were 92.2 percent identical to the calculations performed with Python. The Python program is accurate and fast; therefore, the use is recommended on the field.
Abstract
Similar to other regions, in East Central Europe, agriculture is the most vulnerable sector regarding the consequences of climate change through increasing variability in weather conditions, even on the short-term and local scales. Agricultural engineers make decisions; higher education has a crucial role in taking proper actions. Our survey aimed to get up-to-date information on the knowledge and attitude of graduating students completing agriculture-related studies at 6 universities located in Hungary, the Czech Republic, Poland, and Slovakia, with particular attention to weather projections, crop production, and soil protection issues. Analyses revealed adequate lexical knowledge of young engineers in each country. They are familiar with the agro-environmental actualities and future trends, issues to address at the right time, and the repertoire of tools and practices for taking efficient measures. A positive attitude toward proactive actions was proved. We report proof of a high level of preparedness resulting from the proper efficacy of agricultural higher education. The content of the curricula and the teaching methodologies meet well the receptiveness to learning in the V4 countries. Our findings confirm that frequent updating of the content of subjects as well as incorporating practical applications that promote active learning and engagement, are more critical today than ever, and it is possible to achieve a high level of preparedness for the challenges in the agricultural sector.
